Simultaneous Determination of 37 Kinds of Prohibited Veterinary Drug Residues in Aquacultural “Non-pharmaceutical” Inputs by Ultra Performance Liquid Chromatography－Tandem Mass Spectrometry with Solid Phase Extraction

ZHANG Wei; XIAO Man; WU Dan; HUANG Hao-peng; XU Yuan-yuan; ZHANG Bing; ZHONG Shi-hua

doi:10.19969/j.fxcsxb.22053001

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Simultaneous Determination of 37 Kinds of Prohibited Veterinary Drug Residues in Aquacultural “Non-pharmaceutical” Inputs by Ultra Performance Liquid Chromatography－Tandem Mass Spectrometry with Solid Phase Extraction

Special Column for DRE Thesis Competition | 更新时间：2023-01-04

- Simultaneous Determination of 37 Kinds of Prohibited Veterinary Drug Residues in Aquacultural “Non-pharmaceutical” Inputs by Ultra Performance Liquid Chromatography－Tandem Mass Spectrometry with Solid Phase Extraction
- Journal of Instrumental Analysis Vol. 41, Issue 12, Pages: 1751-1757(2022)
- 作者机构：
  
  1.深圳市质量安全检验检测研究院，广东深圳 518101
  2.广东省市场监督管理局食用农产品监管重点实验室，广东深圳 518101
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.22053001
  CLC：
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张微,肖曼,吴丹等.固相萃取/超高效液相色谱－串联质谱法同时测定水产养殖“非药品”投入品中37种禁限兽药[J].分析测试学报,2022,41(12):1751-1757.

ZHANG Wei,XIAO Man,WU Dan,et al.Simultaneous Determination of 37 Kinds of Prohibited Veterinary Drug Residues in Aquacultural “Non-pharmaceutical” Inputs by Ultra Performance Liquid Chromatography－Tandem Mass Spectrometry with Solid Phase Extraction[J].Journal of Instrumental Analysis,2022,41(12):1751-1757.
张微,肖曼,吴丹等.固相萃取/超高效液相色谱－串联质谱法同时测定水产养殖“非药品”投入品中37种禁限兽药[J].分析测试学报,2022,41(12):1751-1757. DOI： 10.19969/j.fxcsxb.22053001.

ZHANG Wei,XIAO Man,WU Dan,et al.Simultaneous Determination of 37 Kinds of Prohibited Veterinary Drug Residues in Aquacultural “Non-pharmaceutical” Inputs by Ultra Performance Liquid Chromatography－Tandem Mass Spectrometry with Solid Phase Extraction[J].Journal of Instrumental Analysis,2022,41(12):1751-1757. DOI： 10.19969/j.fxcsxb.22053001.

摘要

建立了固相萃取/超高效液相色谱－串联质谱（SPE/UPLC－MS/MS）同时测定水产养殖“非药品”投入品中37种禁限兽药（磺胺类、酰胺醇类、硝基咪唑类、苯并咪唑类、抗病毒类）残留量的分析方法。样品经含0.2%甲酸的80%乙腈水溶液提取，Mcllvaine－乙二胺四乙酸二钠（Mcllvaine－Na,2,EDTA）缓冲液螯合，超声波萃取，Waters PRiME－HLB固相萃取柱净化，通过C,18,色谱柱分离，采用UPLC－MS/MS选择电喷雾ESI离子源在正、负离子多反应监测模式下分析测定，基质添加标准曲线外标法定量。37种禁限兽药标准曲线的相关系数均不低于0.991，检出限为0.156 ~ 1.94 μg/kg，定量下限为0.520 ~ 6.47 μg/kg，加标回收率为71.6% ~ 119%，相对标准偏差为1.2% ~ 15%。该方法快速、准确、灵敏度高，可应用于水产养殖“非药品”投入品中37种禁限兽药残留的快速准确筛查和检测。

Abstract

An ultra performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS） with solid phase extraction was established for the simultaneous determination of 37 kinds of prohibited veterinary drug residues，i.e．sulfonamides，aminools，nitroimidazoles，benzimidazoles and antiviral classes in aquacultural “non-pharmaceutical” inputs．The samples were extracted with 80% acetonitrile aqueous solution containing 0.2% formic acid and chelated with Mcllvaine－Na,2,EDTA buffer，then ultrasonically extracted．The residues contents were separated on a C,18, chromatographic column，then determined by UPLC－MS/MS with electrospray ion source in positive and negative ion mode under multiple reaction monitoring mode．The quantitative information was obtained by matrix-added calibration with external standard．The correlation coefficients of calibration curves for 37 banned veterinary drugs were not less than 0.991．The limits of detection and quantitation were in the range of 0.156－1.94 μg/kg and 0.520－6.47 μg/kg，respectively．The spiked recoveries of the method ranged from 71.6% to 119%，with the relative standard deviations（RSDs） of 1.2%－15%．The method is rapid，accurate and sensitive，and it could be used for the rapid and accurate screening and detection of 37 kinds of prohibited veterinary drug residues in aquacultural “non-pharmaceutical” inputs.

关键词

固相萃取超高效液相色谱－串联质谱“非药品”投入品兽药残留

Keywords

solid phase extractionultra performance liquid chromatography－tandem mass spectrometry （UPLC－MS/MS）“non-pharmaceutical” inputsveterinary drug residue

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